Tetrahydrofuran → HCID 117949317, compound

Participants

Reaction Steps

3-Bromo-1-(3-chloropyridin-2-yl)-N-(2-methyl-6-nitrophenyl)-1H-pyrazole-5-carboxamide prepared in Step 1 (1.27 g, 2.91 mmol), THF (0.2 M, 14.6 mL) and Na2S2O4 (5.37 g, 26.2 mmol, 9.0 eq) were added to a 100 mL round flask and stirred. In a separate flask, NaHCO3 (2.20 g, 26.2 mmol, 9.0 eq) was dissolved in H2O (0.1 M, 29.1 mL) and slowly added to the reaction solution. MeOH (0.6 M, 4.9 mL) was added to the reaction solution, subjected to a reaction at room temperature for 5 minutes, and the solvent was removed therefrom under reduced pressure upon completion of the reaction. The residue was extracted with ethyl acetate (20 mL x 2) and brine (20 mL x 2), and the organic layer thus obtained was dried over MgSO4 and concentrated under reduced pressure. Upon completion of removing the solvent, the residue was dissolved in a small quantity of ethyl acetate, wetted with ethyl acetate/hexane (1:1) and then filtered. The solvent was removed under reduced pressure to obtain the title compound.

Provenance & Evidence